US7314570B2 - Method for removing heavy metals from media containing heavy metals by means of a Lyocell moulded body, cellulosic moulded body comprising absorbed heavy metals, and the use of the same - Google Patents

Method for removing heavy metals from media containing heavy metals by means of a Lyocell moulded body, cellulosic moulded body comprising absorbed heavy metals, and the use of the same Download PDF

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US7314570B2
US7314570B2 US10/487,114 US48711404A US7314570B2 US 7314570 B2 US7314570 B2 US 7314570B2 US 48711404 A US48711404 A US 48711404A US 7314570 B2 US7314570 B2 US 7314570B2
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moulded body
lyocell
cellulosic
heavy metals
body according
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US20050035057A1 (en
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Stefan Zikeli
Thomas Endl
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LL Plant Engineering AG
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ZiAG Plant Engineering GmbH
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28023—Fibres or filaments
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06—Use of materials for tobacco smoke filters
    • A24D3/08—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
    • A24D3/10—Use of materials for tobacco smoke filters of organic materials as carrier or major constituent of cellulose or cellulose derivatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42—Use of materials characterised by their function or physical properties
    • A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
    • B01J39/04—Processes using organic exchangers
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/258—Genetic materials, DNA, RNA, genes, vectors, e.g. plasmids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/30—Compounds of undetermined constitution extracted from natural sources, e.g. Aloe Vera
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • A61L2300/408—Virucides, spermicides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/06—Contaminated groundwater or leachate
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/40—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture or use of photosensitive materials

Definitions

  • the solution of the object is a method for removing heavy metals from media containing heavy metals, whereby the medium containing heavy metals is brought into contact with a Lyocell moulded body.
  • the material from marine animal shells can be used directly. If material from the shells of shrimp or bivalves, lobsters, crustaceans and/or prawn is used, the material must be reduced to small pieces.
  • the quantitative composition of material of marine plants and shells of marine animals is preferably 50% by weight to 50% by weight.
  • material from marine plants is used according to the invention.
  • amino acids such as alanine, arginine, aspartic acid, glutamic acid, glycine, leucine, lysine, serine, threonine, tyrosine, valine and methionine.
  • the material of marine plants and/or shells of marine animals can be fed to a mashing process with simultaneous reduction to small size.
  • the mashing can be carried out either in water, in lye or also in the solvent that is needed for dissolving the cellulose later.
  • the material of marine plants and/or shells of marine animals can be added as a solid, powder or suspension, or also in liquid form.
  • the polymer composition enriched with the material of marine plants and/or shells of marine animals can, in the presence of a derivation agent and/or a solvent known for the dissolving process, be converted into a workable extrusion mass.
  • a further possibility for adding the material of marine plants and/or shells of marine animals is addition during a continuous dissolving process, such as described in EP 356419 and U.S. Pat. Nos. 5,049,690 and 5,330,567.
  • the addition can be carried out discontinuously while maintaining a master batch of the cellulose solution.
  • the material of marine plants and/or shells of marine animals are added continuously.
  • the cellulose solution obtained in this way can be spun using a conventional process, such as dry-jet-wet, wet-spinning, melt blown process, centrifugal pot spinning, funnel spinning or dry spinning.
  • a conventional process such as dry-jet-wet, wet-spinning, melt blown process, centrifugal pot spinning, funnel spinning or dry spinning.
  • the patent specifications U.S. Pat. Nos. 5,589,125 and 5,939,000, as well as EP 0574870 B1 and WO 98/07911 describe spinning processes for manufacturing cellulose fibres according to the NMMO method. Where necessary, the formed moulded bodies are subjected to the conventional aftertreatment processes for chemical fibres for filaments or staple fibres.
  • the cellulosic moulded body is preferably selected from the group consisting of cellulose regenerated moulded bodies, such as carbamate, viscose and Lyocell moulded bodies, particularly preferred, a Lyocell moulded body.
  • Further oxides that can be used are AgO as well as further Ag(I) and Ag(III) oxides, such as Ag 2 O 3 .
  • Further salts that can be used are silver chloride, silver sulphide, silver proteins, silver carbonate, and the soluble silver salts silver acetate, silver sulphate, silver citrate, silver lactate and silver picrate.
  • the cellulosic moulded body according to the invention a plant and/or animal material is added to this body, as described in the preceding. In this way, the result is a very uniform distribution of the at least one heavy metal in the cellulosic moulded body according to the invention.
  • This has the advantage that, on the one hand, a large amount of heavy metal can be introduced into the moulded body and, on the other hand, a very uniform release of the adsorbed heavy metal takes place.
  • the cellulosic moulded body according to the invention can also contain other natural and/or synthetic polymers in addition to cellulose, where these polymers can either be added to the spinning composition or can also be present in mixtures as bi-component and multi-component fibres in a side-by-side, island-in-the-sea or sheath-core configuration.
  • the additional polymer is selected from the group consisting of polyester, polyamide, polyvinyl chloride, cellulose carbamate, cellulose acetate, cupro, viscose, polyacrylonitrile, polyolefin, Teflon, hemp, wool, linen and cotton.
  • the manufacture of the cellulosic moulded body according to the invention can be carried out by means of immersing the manufactured moulded body into an aqueous solution containing heavy metal, separating the aqueous solution containing heavy metal and optionally washing and drying the Lyocell moulded body obtained.
  • the loading processes are carried out for between 1 minute and several hours, depending on the application area.
  • a further possibility for manufacturing the cellulosic moulded body according to the invention if a plant and/or animal material is incorporated in this body, is if first the plant and/or animal material, such as algae material reduced to small pieces and ground, is brought into contact with a heavy metal solution, such as a silver nitrate solution, and the mixture obtained in this way is then sprayed dry, whereby the grinding can take place dry or wet and under normal or high pressure. This material, endowed with heavy metal, can then be incorporated into the cellulosic moulded body according to the invention during the manufacture of this body.
  • a heavy metal solution such as a silver nitrate solution
  • This material can, for example, be sprayed onto a fibrous web for textile, technical or medical use, together with the normally used bonding agent, or alone, during the manufacture of the fibrous web, before the fibrous web is dried and processed into the final product.
  • the ground, spray-dried or damp algae material, loaded with heavy metal, can also be added to the spinning solution for the manufacture of the cellulosic moulded body.
  • the cellulosic moulded body according to the invention is particularly usable as an antibacterial and/or fungicidal material, particularly as an antibacterial fibre, antibacterial fibrous web, hygiene article, medical protective clothing, antibacterial water filter, non-woven, filter material or antibacterial sponge.
  • an antibacterial and/or fungicidal material particularly as an antibacterial fibre, antibacterial fibrous web, hygiene article, medical protective clothing, antibacterial water filter, non-woven, filter material or antibacterial sponge.
  • a further possible use concerns the use as bandaging gauze for burn injuries.
  • the cellulosic moulded body according to the invention is particularly usable as a filtering material for liquid and gaseous media in which pollutants are contained, for example as a cigarette filter to remove heavy metals and other pollutants from the smoke.
  • a cellulosic moulded body according to the invention for example, in the form of modified fibres in a cigarette filter that was loaded with palladium and copper salts, toxic carbon monoxide can be converted into carbon dioxide, in addition to the removal of heavy metals from the smoke.
  • This catalyst effect of copper and palladium salts in an aqueous solution, in order to oxidize carbon monoxide into carbon dioxide or sulphur dioxide into sulphur trioxide is described in U.S. Pat. No. 3,790,662.
  • Ring spun yarns carded or combed, that can either be manufactured purely of Lyocell or of different combinations with cotton, silk, linen, microfibres and/or viscose;
  • OE yarns which can either be manufactured purely of Lyocell or of different combinations with cotton, wool, linen and/or viscose;
  • Filament-effect yarns which include sable, terry, shaded and slub yarns, and that can either be manufactured purely of Lyocell or of different combinations with polyester, polyamide, viscose and/or Trevira CS;
  • Filament yarns flat, textured or high-twist, that can either be manufactured purely of Lyocell or of different combinations with acetate, triacetate, polyester, polyamide and/or viscose;
  • Technical yarns which include, for example, Parafil Plyfil or Corespun, and that can either be manufactured purely of Lyocell or of different combinations with Kevlar, Preox, Nomex, Kermel, carbon, glass, steel, viscose and/or polyester; and
  • Elastic yarns which include, for example, wrap yarn, Siro, Plyfil or Corespun, and that can either be manufactured purely of Lyocell or of different combinations with cotton, shear wool, polyester, linen, elasthan and/or viscose.
  • the combinations with other fibres have the advantage that the product's wearing comfort and properties for hygienic applications and clothing can be adjusted using mixture components.
  • the antibacterial properties or ion exchange properties are not impaired by this.
  • These yarns can be processed into fabrics using, for example, shuttle, rapier, projectile or jet machines, which, for example, are extremely well suited for the application areas of ion exchange and antibacterial properties.
  • the yarns can be processed into knitted fabrics using flat bed, single jersey, double knit and warp knit machines, which are likewise extremely well suited for the application areas of ion exchange and antibacterial properties.
  • the Lyocell moulded bodies according to the invention can be further processed into endless or cut form to non-woven products for industrial uses, such as roofing materials, separators, filters, reinforcing basic bodies, sealing materials and insulating materials, for special papers such as dust filters, filters for waste and/or process waters, sausage casings, for textile applications such as medical applications (swabs and gauze), wadding, stockings, shoe inserts, shoe inner lining, bedding, home textiles, serviettes, washing clothes, paper towels or nappies.
  • roofing materials such as roofing materials, separators, filters, reinforcing basic bodies, sealing materials and insulating materials
  • special papers such as dust filters, filters for waste and/or process waters
  • sausage casings for textile applications such as medical applications (swabs and gauze), wadding, stockings, shoe inserts, shoe inner lining, bedding, home textiles, serviettes, washing clothes, paper towels or nappies.
  • the fabrication can either be processed into pure Lyocell products or in combination with other fibres, with super absorbers, with activated carbon and with native cellulose (fluff cellulose) in order to achieve a combination effect.
  • combinations with super absorbers display extremely high absorption of water;
  • the combination with activated carbon in granulate or fibre form also shows, in addition to an antibacterial effect and an ion exchange effect, an extra capability of adsorbing organic materials and/or colouring substances.
  • bonding agents such as latex polymers, diethylene, butadiene, vinyl acetate and/or styrenes
  • bonding agents are preferably added in an amount of from 1-30% by weight.
  • thickeners, catalysts, filler materials, colouring substances, lubricants, optical bleaching agents and/or defoamers can be added.
  • the manufacture of the non-wovens or fibrous webs can take place using a carding, wetlaid, airlaid or extrusion process.
  • the fibrous webs manufactured in this way can be compacted by means of needlepunch, stitch bond, hydroentanglement, spun bond or melt blowing treatment. Additional possibilities are chemical compaction with a corresponding bonding agent or thermal compaction or the admixing of thermoplastic additives, which are compacted into a fibrous web with the cellulosic fibres.
  • the non-woven products can additionally be chemically and/or mechanically treated, in order, for example, to optimize moisture absorption and moisture transport, or to improve the absorption capability, fire resistance, electrical resistance, friction properties and/or abrasion properties.
  • calendering suede finishing, raising the nap, polishing, shearing and brushing or combing.
  • Further aftertreatment techniques are lamination, embossing and profiling using a calender or creping.
  • the non-woven products can be constructed in one or more layers and present a typical mass per unit area from 15-500 g/m 2 .
  • the cellulosic moulded bodies can find application in the form of antibacterial sponges or sponge wipes.
  • a moulded body, according to the invention and with antibacterial effect is manufactured by adding a heavy metal, in metallic, ionic or complexed form, during an extra process step, for example either before or after the drying.
  • Preferred embodiments can be derived from the following examples.
  • Lyocell sponges according to the invention can be obtained as described in WO 99/27835.
  • a pore-forming agent and fibre reinforcement are mixed in with the N-oxide water cellulose solution and the mass is applied to a conveyor belt using sheeting dies. The sedimentation takes place in a warm spinning bath in order to liquefy and dissolve the pore-forming agent.
  • One variant is application of the N-oxide water cellulose solution to a plastic net. No blowing agent is used, so that neither the mechanical stability nor a corresponding abrasion. resistance of the sponge or sponge wipe can be achieved.
  • WO 99/27835 describes impregnation of the sponges with substances with a biocide effect, such as isothiazolon, benzimidazole derivatives, tertiary ammonia salts, zeolites, glycerine and propylene glycol.
  • a further method for manufacturing Lyocell sponges according to the invention is similarly described in WO 97/23552.
  • a cellulose solution of an aqueous amine oxide is mixed with a pore-forming agent (an alkaline salt or alkaline earth salt or an inorganic acid, e.g., Na 2 SO 4 ) and a blowing agent.
  • a pore-forming agent an alkaline salt or alkaline earth salt or an inorganic acid, e.g., Na 2 SO 4
  • the mass is subjected to conditions that lead to decomposition of the blowing agent and therefore to a foaming of the cellulose solution.
  • the foamed cellulose solution is brought into contact with water in order to precipitate the cellulose and wash out the pore-forming agent.
  • a Lyocell sponge according to the invention with an antibacterial effect, is manufactured by adding a heavy metal in metallic, ionic or complexed form, during an extra process step either before or after the drying.
  • the detailed embodiment can be derived from the following examples.
  • Carbamate sponges according to the invention can be manufactured analogously to the method described in JP21172302, whereby again heavy metal is added at any stage of the process, preferably again before or after the sponge is dried.
  • the fibres were cut to a fibre staple of 40 mm, washed without solvent and given a 10 g/l softening (50% Leomin OR-50% Leomin WG (fatty acid polyglycol ester containing nitrogen, from the company Clariant GmbH)) at 45° C. or the fat overlay for improved further processing of the fibre was applied and dried at 105° C.
  • a 10 g/l softening 50% Leomin OR-50% Leomin WG (fatty acid polyglycol ester containing nitrogen, from the company Clariant GmbH)
  • Table 1 shows that the spinning characteristics of the spinning solution obtained according to this example were good.
  • Lyocell cellulose fibres were continuously manufactured according to Example 1, whereby the respective amount, the conditions of the continuously maintained process and the physical properties of the fibres obtained are listed in the following Table 2. 8% brown algae material, referred to the cellulose, was used.
  • Table 2 presents the fibre data for the modified Lyocell fibre.
  • Lyocell fibres were continuously manufactured according to Example 1, with the difference that no brown algae material was added.
  • the metal ion content was determined according to the testing method:
  • the fibre material was filtered by suction and washed with completely demineralised water until no more silver traces (test with a NaCl solution) were detected.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre obtained in this way was analysed for its silver content.
  • 1N nitric acid (1 hour) was added in order to dissolve the silver.
  • the nitric acid solution was filtered off and then titrated with 0.1 N NaCl. To improve the visibility of the end point of the titration, the filtrate was heated so that the resulting precipitate agglomerated.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre material was filtered by suction and washed with completely demineralised water.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • Example 2 Example 3 [mg/kg fibre] [mmol/kg fibre] [mg/kg fibre] [mmol/kg fibre] [mmol/kg fibre] Example 4 Silver 1855 17.2 237 2.2 Example 5 Copper 899 14.2 591 9.3 Example 6 Zinc 756 11.6 526 8.0 Example 7 Mercury 9460 47.2 376 1.9 Example 8 Tin 1670 14.1 1030 8.7 Example 9 Cadmium 1270 11.3 793 7.1 Example Silver 1410 13.1 207 1.9 10 Example Arsenic 170 2.3 72 1.0 11 Example Lead 2720 13.1 1790 8.6 12 Example Antimony 496 4.1 267 2.2 13
  • Lyocell fibres present a high adsorption capacity, and that this adsorption capacity can be increased by another 50% with the modified Lyocell fibres.
  • the fibres produced according to Example 4 were then examined for bacterial resistance.
  • the bacteria were furthermore applied to fibre material from Example 1 and, as a growth control, standard cotton was subjected to the same test treatment.
  • the bacterial growth inhibiting or bacterial reduction activity is determined from the bacterial content (the number of colony-forming units—CFU) in the sample and the control.
  • an anode of raw silver is subjected to electrolytic refining in conventional Moebius cells.
  • silver nitrate as an electrolyte, is used at a concentration of 5-80 g/l of silver at a temperature of 40° C. While it is true that the electrolyte is constantly reused, nevertheless, during maintenance work and standstills, waste waters with silver concentrations that are also partially less than in the electrolyte do occur.
  • the recovery of the silver nitrate by means of the Lyocell moulded body according to the invention was tested using a synthetic silver nitrate solution. 2 kg of fibre from Example 2 were filled into a 5 l PP pressure tank with backup plate.
  • the fibre was subsequently moistened with 5 l of completely demineralised water.
  • 10 l of silver nitrate, at a concentration of approximately 1 g Ag/l, were introduced into a PP container.
  • this quantity was pumped over the pressure tank (with the moistened fibres from Example 3) to recirculate.
  • a recirculation flow rate of 30 l/h was selected.
  • FIG. 1 is a graphic representation of the results obtained in this example.
  • the fibre material was filtered by suction and washed with completely demineralised water until no more silver traces (test with a NaCl solution) were detected.
  • the fibres were dried in a circulating air drying cabinet at approximately 105° C.
  • the fibre obtained in this way was analyzed for its silver content.
  • N nitric acid was added (1 hour) in order to dissolve the silver.
  • the nitric acid solution was filtered off and then titrated with 0.1 N NaCl. To improve the visibility of the end point of the titration, the filtrate was heated so that the resulting precipitate agglomerated.
  • the fibres produced according to Example 17 were then examined for bacterial resistance.
  • the bacteria were applied to fibre material from Example 17 and, as a growth control, standard cotton and cellulose were subjected to the same test treatment.
  • the bacterial growth inhibiting or bacterial reduction activity is determined from the bacterial content (the number of colony-forming units—CFU) in the sample and the control.
  • the difference is formed between the base-10 logarithms of the number of colony forming units (CFU) in the control sample and the sample, each after 18 hours of incubation.
  • Example 2 The washing out characteristics of a Lyocell fibre with algae incorporation (Example 2) treated according to Example 10 (with 0.1 M AgNO 3 ) was tested in the following way:
  • a card sliver was produced from this mixture for homogenization purposes, and this card sliver was examined for antibacterial properties according to Example 18.
  • the levels after 18 hours of incubation are specified for the standard cotton and cellulose as a growth control and for the modified Lyocell fibre produced according to Example 22.
  • a card sliver was produced from this mixture for homogenization purposes, and this card sliver was examined for antibacterial properties according to Example 18.
  • the levels after 18 hours of incubation are specified for the standard cotton and cellulose as a growth control and for the modified Lyocell fibre produced according to Example 22.
  • a card sliver was produced from this mixture for homogenization purposes, and this card sliver was examined for antibacterial properties according to Example 18.
  • the levels after 18 hours of incubation are specified for the standard cotton and cellulose as a growth control and for the modified Lyocell fibre produced according to Example 22.
  • the fibres were cut to a fibre staple of 40 mm, washed without solvent and given a 10 g/l softening (50% Leomin OR-50% Leomin WG (fatty acid polyglycol ester containing nitrogen, from the company Clariant GmbH)) at 45° C. or the fat overlay was applied for improved further processing of the fibre and dried at 105° C.
  • the mass was filled into a perforated form and placed for 30 minutes into a first precipitation bath that was at a temperature of 95° C. and that contained 10 g/l of sodium carbonate and 80 g/l of sodium sulphate.
  • the pre-precipitated mass was transferred to a second bath for 15 minutes; this bath's temperature was 60° C. and it contained 70 g/l sulphuric acid and 140 g/l sodium sulphate, in order to completely regenerate the cellulose.
  • the sponge is produced analogously to Example 27, whereby an additional 8 g of brown algae powder, finely reduced to small pieces, was added to the viscose solution.
  • the dried and desulphurised sponge was then transferred to a bath of 0.1 N silver nitrate and left in the bath for approximately 1 hour.
  • the sponge containing Ag was then washed free and dried again.
  • the sponge was examined for antibacterial properties.
  • the bacteria were applied to the sponge and, as a growth control, the standard sponge from Example 27 was subjected to the same test treatment.
  • the bacterial growth inhibiting or bacterial reduction activity is determined from the bacterial content (the number of colony-forming units—CFU) from the sample and the control.
  • a sponge was produced analogously to Example 27. There was, however, no addition of algae powder and no addition of viscose short cut fibres; instead, 35 g of a short cut Lyocell fibre with incorporated algae (12% algae referred to the cellulose—produced according to WO 01/62844) was added. A sponge was produced analogously to Example 28 and treated with silver nitrate.
  • This sponge also displayed a strong antibacterial effect.
  • cellulose carbamate To produce cellulose carbamate, first an alkali cellulose was produced from the chemical cellulose Borregaard SVS. The caustic soda solution was washed out of the processed alkali cellulose (35% cellulose by weight; 15% NaOH by weight; 50% water by weight) with water. After the cellulose (70% water by weight) activated in this way was squeezed out, 10 kg of the squeezed activated cellulose were mixed with carbamide (1.5 kg) in a kneading machine. In this process, the carbamide present in the water in the cellulose dissolved and was uniformly distributed in the cellulose.
  • This cellulose pulp was transferred to a reactor, which was equipped with a mixer and reflux cooler, and which already contained o-xylene (35 kg). The reactor contents were then heated to 145° C. for approximately 2 hours and then filtered off.
  • a sponge was produced analogously to Example 31, but there was no addition of algae powder; instead, approximately 11 g of treated algae powder was added.
  • This sponge also displayed a strong antibacterial effect.
  • This sponge also displayed a strong antibacterial effect.
  • a sponge was produced analogously to Example 35, but there was no addition of algae powder during the production of the solution; instead, approximately 25 g of treated algae powder was added along with the addition of the pore-forming agent and short cut fibres.
  • the bacterial growth inhibiting or bacterial reduction activity is determined from the bacterial content (the number of colony-forming units—CFU) in the sample and the control.

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US10/487,114 2001-08-20 2001-11-29 Method for removing heavy metals from media containing heavy metals by means of a Lyocell moulded body, cellulosic moulded body comprising absorbed heavy metals, and the use of the same Expired - Fee Related US7314570B2 (en)

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DE10140772A DE10140772A1 (de) 2001-08-20 2001-08-20 Verfahren zur Entfernung von Schwermetallen aus schwermetallhaltigen Medien unter Verwendung eines Lyocell-Formkörpers sowie Lyocell-Formkörper mit adsorbierten Schwermetallen und deren Verwendung
DE10140772.6 2001-08-20
PCT/EP2001/013970 WO2003018166A1 (fr) 2001-08-20 2001-11-29 Procede de retrait de metaux lourds contenus dans des substances comprenant des metaux lourds au moyen d'un corps moule en lyocell, corps moule cellulosique ayant adsorbe des metaux lourds et son utilisation

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DE10140772A1 (de) 2003-03-13
EP1418996A1 (fr) 2004-05-19
ZA200400851B (en) 2004-10-22

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